Modular reactor system with stirrer

ABSTRACT

A modular reactor system comprises a backplane connected to a computer and a thermal control unit. The backplane includes a plurality of seats for releasably holding a plurality of modules. Each module holds a reactor vessel that may be used to conduct experiments. A plurality of laboratory instruments, such as motors, switches, sensors and pumps are included within the backplane and on the reactor modules. These laboratory instruments are utilized to perform work on the contents of the reactor vessels when the modules holding the reactor vessels are positioned in the backplane. A computer is connected to the backplane and controls the laboratory instruments within the backplane and on the reactor modules positioned within the backplane. A thermal control unit provides a thermal control fluid that is delivered to the reactors in the reactor modules when the modules are properly seated in the backplane.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation of U.S. application Ser. No.10/339,229 filed Jan. 9, 2003.

BACKGROUND

The present invention is related to the field of chemical reactors, andmore particularly, automated reactors for use in process research anddevelopment as may be conducted in a laboratory.

Laboratory automation developed over the past decade has allowedchemists to become much more efficient in conducting experiments.Laboratory automation has been particularly useful for high thru-putscreening, where a large number of different compounds are tested usingparticular chemicals. These tests are typically conducted in very smallreaction vessels, such as multiple well microplates (e.g., 96 wellmicroplates), where a very small amount of reagent is added to a smallamount of experimental solution in each microplate well. From the largenumber of small scale experiments, a few promising leads may beidentified. These leads will require additional testing on a largerscale, before truly promising chemical combinations can be identified.Larger scale testing typically involves larger amounts of experimentalsolution combined with larger amounts of reagents. Of course, thesetests are conducted in larger reaction vessels, such as vessels of 50 mlor more.

A few systems exist that allow chemists to automate experiments inlarger reaction vessels. Examples of such systems include the CLARKE®automatic reactor system sold by Argonaut Technologies, Inc. of FosterCity, Calif. Such systems typically provide a single reactor vessel anda number of laboratory instruments capable of automatically interactingwith the reactor vessel. When using these systems, a chemist firstprepares a reactor and attaches all necessary components for completionof the experiment (e.g., reagent feed lines, temperature sensors,stirrers, etc.). After the reactor is prepared, the chemist uses asoftware program to provide instructions for conducting the experimentusing the laboratory instruments. After receiving the chemist'sinstructions, the software controls the laboratory instruments toautomatically conduct the experiment (e.g., the system automaticallyfeeds reagents at the desired times, monitors reaction variables, stirsthe experimental solution, etc.). This automation allows the experimentto be conducted without the chemist being physically present, thusfreeing the chemist to complete other valuable tasks.

Although laboratory automation continues to assist with high thru-putscreening, many areas for improvement remain. For example, manyautomated laboratory systems for larger scale reactions are limited touse in a single experiment. Chemists would like to simultaneouslyconduct several different larger scale experiments using a singlesoftware program. Furthermore, those automated laboratory systems thatallow chemists to conduct more than one experiment are limited toconducting very similar experiments with similar functions,environmental conditions, and steps in any given batch of experiments.Chemists would like to have the flexibility to simultaneously conductvery different experiments using a single automated laboratory system.Of course, many other areas for improvement remain. The modular reactorsystem of the present invention presents a number of improvements oversuch prior art systems.

SUMMARY

A modular reactor system includes an apparatus that houses several smallreactors and independently measures and controls the critical parametersof each reactor during experiments, thereby allowing chemists to studythe synthesis of a broad range of compounds. The apparatus comprises acomputer, a housing having a plurality of seats, and a thermal controlunit. A plurality of modules are removably positioned in the seats ofthe housing. Each of the plurality of modules includes a module shellthat holds a jacketed reactor vessel. The reactor vessel includes areactor chamber and a plurality of ports leading to the reactor chamberand designed to receive laboratory instruments. Each reactor vessel alsoincludes a fluid chamber formed between an exterior wall and an interiorwall. The exterior wall includes an inlet port for receiving thermalcontrol fluid into the fluid chamber and an outlet port for expellingthermal control fluid from the thermal control chamber for return to thethermal control unit.

The housing of the modular reactor system comprises a trunk thatsupports the plurality of seats and a top canopy. A plurality oflaboratory instruments are positioned within the housing. For example, aplurality of electric motors are connected to stirrers that extend intoreactor vessels seated in the housing. In addition, a plurality of gaslines are positioned in the housing along with a plurality of gas lineconnectors. Each gas line connector joins one of the gas lines to one ofthe modules when the module is positioned in one of the seats of thehousing. Furthermore, a plurality of electrical connectors areassociated with each seat of the housing. Placement of one of themodules in a seat of the housing joins the electrical connector to themodule. The electrical connector provides an electrical connectionbetween the module and the computer.

Each module of the module reactor system further comprises at least oneclamp that retains the reactor in the reactor seat. In addition, eachmodule includes at least one pump positioned on the module shell. Atleast one reagent seat is also positioned on the module shell. The atleast one pump is operable to pump a reagent positioned on the reagentseat to the reactor chamber.

Each module may also include a unique identification. The uniqueidentification may be as simple as a name or tag assigned to the moduleand marked somewhere on the module so that the unique identification maybe read by a human. However, in one embodiment of the invention, theunique identification is an electronic tag or similar identifier. Inthis embodiment, an identification reader is associated with each of theseats. Each identification reader is operable to read the identificationof one of the modules placed in the seat associated with theidentification reader. The unique identification of each module ispassed on to the computer which is programmed to execute uniqueinstructions with respect to each module, regardless of the seat inwhich the module is placed.

These and other features, aspects, and configurations of the presentinvention will become better understood with reference to the followingdescription and the appended claims.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 shows a block diagram of a modular reactor system;

FIG. 2 shows an elevational view of a plurality of modules installed ina backplane unit of the modular reactor system of FIG. 1;

FIG. 3 shows the backplane of FIG. 2 with no modules installed;

FIG. 4A shows a motor installed in the backplane of FIG. 3;

FIG. 4B shows a mount used with the motor of FIG. 4A;

FIG. 5 shows a block diagram of a control board for the modular reactorsystem;

FIG. 6 shows a block diagram of various connections between the controlboard of FIG. 7 and various laboratory instruments;

FIG. 7 shows a front perspective view of one of the modules of FIG. 2;

FIG. 8 shows a side view of the module of FIG. 7;

FIG. 9 shows a back perspective view of the module of FIG. 7;

FIG. 10A shows an elevational view of an exemplary reactor for use withthe modular reactor system;

FIG. 10B shows a parts view of a quick connect attachment for thereactor of FIG. 10A;

FIG. 10C shows a thermal control system for use in the modular reactorsystem of FIG. 1;

FIG. 10D shows a reactor thermal control system for use in the thermalcontrol system of FIG. 10C;

FIG. 11A shows an overview screen of a graphical user desktop of themodular reactor system;

FIG. 11B shows a more detailed overview screen accessible from theoverview screen of FIG. 11A;

FIG. 12 shows a dialog box associated with the graphical user desktop ofFIG. 11;

FIG. 13 shows a stage details screen of a recipe editor of the modularreactor system; and

FIG. 14 shows a stages overview screen of the recipe editor of themodular reactor system;

FIG. 15 shows a configuration screen associated with the graphical userdesktop of FIG. 11A or 11B;

FIG. 16 shows a bottom view of a reactor clamp for use in associationwith the module of FIG. 7;

FIG. 17 shows a perspective view of a rear member of the reactor clampof FIG. 16;

FIG. 18 shows a front perspective view and a rear perspective view of afront member of the reactor clamp of FIG. 16;

FIG. 19 shows a cross-section of the front member of FIG. 18;

FIG. 20 shows a representation of the position of a reactor lid and areactor mouth when the pressure in the reactor vessel is below athreshold pressure;

FIG. 21 shows a representation of the position of the reactor lid andthe reactor mouth when the pressure in the reactor vessel is above thethreshold pressure;

FIG. 22 shows a side view of a reactor lid;

FIG. 23 shows a top view of the reactor lid of FIG. 22.

DESCRIPTION

Overview

With reference to FIGS. 1 and 2, a modular reactor system 10 comprises asupport housing or chassis 12 capable of releasably holding multiplereactor modules 16 (also referred to herein as simply “modules”). Aplurality of module seats are provided for holding the reactor modules16. Each reactor module 16 holds a reactor vessel 30 that may be used toconduct experiments. A plurality of laboratory instruments, such asmotors, switches, sensors and pumps are included within the supporthousing 12 and associated with each seat of the support housing. Aplurality of laboratory instruments are also provided on each of thereactor modules 16. These laboratory instruments are utilized to performwork on the contents of the reactor vessels 30 when the modules 16holding the reactor vessels 30 are positioned in the support housing 12.The support housing 12 is also referred to herein as the “backplane”, asit provides the background platform for one or more laboratoryinstruments and/or module 16 connections. A computer 18 is connected tothe backplane, and the laboratory instruments within the backplane 12are in communication with the computer 18. Laboratory instruments on thereactor modules 16 are in communication with the computer 18 when thereactor modules are positioned within the backplane 12. Each laboratoryinstrument may be independently controlled by the computer, regardlessof the seat or module associated with the laboratory instrument. To thisend, a first laboratory instrument associated with one module or seatmay be activated without activation of a similar laboratory instrumentassociated with a different module or seat. A thermal control unit 14includes a plurality of individual reactor thermal control systems 13and a chill fluid system 14A. As described in further detail herein, theindividual reactor thermal control systems 13 work with the chill fluidsystem to provide thermal control fluid to the reactors in the reactormodules when the modules are properly seated in the backplane. Thecomputer 18 is also in communication with the thermal control unit 14,and the thermal control unit is arranged to provide independenttemperature control for each reactor vessel in each module.

Backplane

With reference to FIG. 3, the backplane 12 includes a plurality ofmodule seats 20 designed to releasably hold the reactor modules 16. Theterm “slot” is also used herein to refer to a module seat 20. Each slot20 is defined by two module guide rails 21. The module guide rails 21are sized to receive a base portion 83 of one of the reactor modules 16(see FIG. 9). The module guide rails include slits extending along theguide rails that are designed to receive a lip 81 on the module base 83(see FIG. 9). Pinion gears may be included along the side rails andslits in order to mesh with a slotted rack on the lips of the module.This rack and pinion mechanism provides for smooth insertion of themodules into the slots 20 of the backplane 12. A crank device ormechanism that drives the pinion gears (not shown) may also be providedin association with each slot to assist with full insertion of themodule into the slot. For example, the crank device may be activated topull the module further into the slot using the slotted rack on the lips81 of the module. In one embodiment, access to the crank device could beprovided through holes 25 located at the base of the backplane, and thecrank device may be rotated using a screwdriver or similar elongatedrotation device.

A plurality of electrical connectors 40 are positioned in the backplaneabove the slots 20, such that each electrical connector is associatedwith one of the slots. Each electrical connector 40 is designed to matewith an electrical connector on a reactor module 16 when the reactormodule is placed in the slot. Gas line connections 41, two fluid ports23, and a backlight 25 are also provided directly above each slot 20.The gas line connectors 41 are designed to mate with gas line connectorson each module. The gas line connectors 41 not only provide a connectionbetween the modules and the gas lines in the backplane, but also providea connection to a vacuum and/or pressure source also located in thebackplane. The fluid ports 23 provide a connection to the fluidcirculated in the thermal control unit. The backlights 25 provide alight source to assist with viewing the contents of the reactors whenmodules holding the reactors are seated in the backplane. Furthermore,an identification reader 22 in the form of an electric tag reader isprovided in each slot. The identification reader 22 is positioned withinthe slot to read an identification placed on one of the modules that isplaced in the slot. The identification on each module is an electronictag that can be read by the electronic tag reader 22.

The backplane 12 also includes a top canopy 45 that sits above the slots20. The top canopy 45 includes a front panel 42 that includes a numberof input/output devices related to the laboratory instruments. Inparticular, the front panel 42 includes a number of receptacles 44 usedto receive electronic information from laboratoryinstruments/transducers included on the reactor modules. For example,receptacles 44 are provided for receiving measurements/signals relatedto temperature, such as the temperature of the reactor contents, thetemperature of the vapor within the reactor, and/or the temperature ofthe ambient air. A receptacle 44 is also provided for receivingmeasurements/signals indicating the pH level of the reactor contents.Furthermore, an auxiliary receptacle 44 is provided for receiving otherelectronic signals/measurements related to the reactor. For example, theauxiliary receptacle could be used with a sensor to measure and/orcontrol the pressure within the reactor or the volume of fluid withinthe reactor. The receptacles 44 are positioned on the top panel 42 insets associated with each slot.

Gas flow knobs 48 are also provided on the top panel 42. One gas flowknob 48 exists for each slot of the backplane. Each of the gas flowknobs 48 controls a valve in a gas line located in the backplane 12 thatis fed with inert gas from a delivery manifold connected to a large tank(not shown) positioned exterior the backplane. The gas lines in thebackplane 12 direct gas between the tank and the gas line connectors 41associated with the slots 20. Accordingly, an inert gas can be directedto each module 16 placed in the backplane. Turning the knobs 48 willcontrol the valves to allow more or less gas to flow through the gaslines in the backplane. A plurality of bubbler path switches 38 are alsoprovided for each gas line in the backplane. If one of the bubbler pathswitches 38 is activated, the flow of the inert gas to a particularmodule is directed through a reactor bubbler 39 located directly abovethe slot 20 holding the module 16. The bubbler 39 provides a visualindication of the amount of gas flowing through the gas line in thehousing to the module. A system bubbler 43 is also provided to provide avisual indication that the gas in the delivery manifold is beingrefreshed.

A vent port 46 is provided above each slot 20, next to each set ofreceptacles. A tube from the reactor vessel 30 to the vent port 46 maybe used to vent the inert gas and/or reaction fumes away from thereactor vessel. This vent port 46 includes a valve and pressuretransducer that can be closed to measure reactor pressure. To this end,the backplane is typically placed in a laboratory hood (not shown) sothat gasses and fumes leaving the reactor vessels are vented out of thelaboratory through the hood. At the same time, a clean air inlet 35 isprovided into the backplane. This inlet 35 provides a source of cleanair that may be used to purge or dilute other gasses within thebackplane or those created during an experimental process.

In addition to those discussed above, a number of other I/O devices maybe provided on the top panel or elsewhere on the backplane 12. Forexample, output devices such as LEDs and other display means could beprovided to indicate temperature warnings (e.g., excessive temperaturewarning) or instrument operation (e.g., coolant is flowing).

A variety of laboratory instruments may also be included in thebackplane under the top canopy 45 and behind the top panel 42 above eachslot. For example, a robotic arm (not shown) may be provided under thetop canopy 45 of the backplane. Of course, the instruments in thebackplane 12 may be mounted on other locations of the backplane and donot need to be mounted under the top canopy 45 and/or behind top panel42. The robotic arm may be used to accomplish tasks that may benecessary during any particular experiment, such as taking samples froma particular reactor.

Other instruments which may be included in the backplane are electricmotors. For example, according to one embodiment, electric motors usedfor stirrers are mounted behind top panel 42 above each slot. Theseelectric motors may be connected to stirring shafts that extend into thereaction vessels 30 when the modules 16 are placed in the slots 20 ofthe backplane 12. The electric motors are not shown in FIG. 3, but theposition of an electric motor behind the backplane is indicated byreference numeral 47. A view of a motor 130 positioned under the topcanopy 45 is shown in FIG. 4. The motor 130 is held within a mount 132that is connected to the backplane 12. The motor includes driveshaft 134that is connected to a stirrer shaft 79 by a quick connect device 136.

Because the reactor vessel 30 is not permanently attached to thebackplane 12, misalignment between the reactor vessel 30 and thestirring shaft 79 may occur. One way that known systems compensate forthis misalignment is through the use of spring couplers. Anotherapproach relies upon the use of a flexible tube in line between theshaft 79 of the stirrer motor and a Teflon® coated shaft which extendsinto the reactor. Both of these solutions, however, create additionalproblems. For example, both solutions result in side loading of theshaft. Accordingly, removal of the stir shaft is made more difficult.Moreover, the side loading on the shaft results in wear of the shaftand/or the seal at the point the shaft enters the reactor. This wear mayresult in contamination of the reaction mixture, loss of pressurecontrol in the reactor, or even shaft failure.

According to one embodiment of the modular reactor system, a stirrersystem is provided which avoids the problems associated with knownsystems by allowing for the effect of movement of the stirrer system inthe X-Y plane. Referring to FIG. 4B, one embodiment of a stirrer systemis further described. Motor 130 is attached to mount 132. Mount 132comprises counter-balance arms 150 and 152. Mount 132 is pivotablyconnected to rotatable base 154 by a pin which is inserted through hole156. Rotatable base 154 is fixedly connected to shaft 158. Also shown inFIG. 4B is telescoping shaft 160 which is internally shaped so as toreceive universal ball 162 which is fixedly connected to stirrer shaft79. The telescoping shaft 160 may also be referred to herein as atelescoping portion of the stirrer shaft 79. The connection of thetelescoping shaft 160 to the stirrer shaft 79 using the universal ball162 may also be referred to herein as a universal joint.

To connect telescoping shaft 160 to universal ball 162, an operatorpulls telescoping shaft 160 downward until it nears universal ball 162.If universal ball 162 and telescoping shaft 160 are misaligned, theoperator may rotate shaft 158 to obtain rotation about axis A, havingthe effect of moving the telescoping shaft along the X-axis.Alternatively and/or additionally, the operator may pivot motor mount132 about the pin inserted in hole 156, resulting in motion about axisB, having the effect of moving the telescoping shaft along the Y-axis.Thus, telescoping shaft 160 may be positioned over universal ball 162such that when telescoping shaft 160 is turned by motor 130, universalball 162 and stirrer shaft 79 are caused to rotate. According to oneembodiment, counterbalance arms 150 and 152 are movable, such thattelescoping shaft 160 may be positioned near universal ball 162 bymoving counterbalance arms 150 and 152.

Those of skill in the relevant art will recognize that a number ofalternative embodiments exist for the stirrer system of the presentinvention. By way of example, but not of limitation, the ball may belocated on the motor shaft. Alternatively, a third piece may be usedwhich provides coupling between the motor shaft and the stirrer shaft.Moreover, springs may be used to bias the coupling means. This isuseful, for example, for embodiments wherein it is desired to makecoupling of the motor shaft to the stirrer shaft automatic uponinsertion of the reactor module into the backplane. A number ofalternative embodiments are also possible regarding the counterbalancearms. By way of example, but not of limitation, the counterbalance armsmay be movable about a plurality of axes. According to anotherembodiment, the location of the motor within the mount serves tocounterbalance the system. The salient characteristic is the ability tominimize side loading of the stirrer shaft when the alignment betweenthe stirrer shaft and the motor shaft is varied.

With reference again to FIG. 3, the backplane further includes a trunk15 that acts as the housing for electric wiring, gas lines, and theelectronics box for the backplane. The top canopy 45 and the slots 20are connected to and supported by the trunk 15 of the backplane. Thetrunk 15 includes a power inlet 17 for receiving a power cord. The trunkalso includes a power switch 19. In addition, the trunk 15 includesvacuum switches 27 that are operable to turn on or off the vacuumprovided to each slot of the backplane. Furthermore, a main gas supplyconnection 29 is provided through the trunk 15. This connection allows agas line to be easily connected to the backplane, so the gas can beprovided to each slot and module positioned within the backplane.

A control board 50 is positioned within the trunk 15 of the backplane12. With reference to FIG. 5, the control board 50 is a circuit boardthat serves as the interconnection between the computer 18 and theelectronic instruments within the backplane. A standard RS-232 interfaceis used to connect the computer 18 to the control board. This connectionmay be a direct connection, connection over a local area network, oreven a wide area network. The control board 50 includes a processor 54that communicates with software on the computer 18 to control allinstruments and output devices connected to the backplane 12.Furthermore, the processor 54 receives information from various sensorsand other system inputs through the backplane 12 and passes theinformation on to the computer 18 at designated times.

As shown in FIG. 5, the processor 54 is powered by power supply 56. Theprocessor 54 is connected to global I/O unit 58 through bus 59. Theglobal I/O unit 58 transfers signals to and receives signals from theI/O devices on the backplane that are not associated with a particularmodule. For example, the global I/O unit 58 receives signals related tothe presence of a vacuum at vacuum switch 27, the flow of gas through amain gas line, the flow of fluid through the thermal control unit 14,the temperature of the fluid, the ambient air temperature, and theinternal temperature of the backplane. The global I/O unit 58 alsocontrols the state of the backlights associated with each slot of thebackplane. The processor 54 is further connected to a number ofdedicated module control units 60, user I/O units 62 and module ID units22 (referenced above as “identification readers”) through bus 61. Themodule control units 60 transfer control signals to particular modules16 positioned in the slots 20 of the backplane 12, and receive inputsrelated to the particular modules. For example, one of the modulecontrol units 60 may relay signals instructing one of the motors 130 tospin, thereby operating the stirrer connected to the motor. As anotherexample, one of the module control units 60 may receive a temperatureinput from one of the modules that is then passed on to the processor 54and computer 18.

FIG. 6 shows the connection between a module control unit 60 and variouslaboratory instruments associated with a particular module 16. Forexample, readings from temperature probes 140, a pressure probe 144, apH probe 142, and a module detect 146 are all delivered to the modulecontrol 60. In addition, the module control unit 60 provides controlsignals to the reagent feed pumps 86 positioned on the module. Themodule control unit 60 also controls various valves 147 within thebackplane, such as gas valves, vacuum valves, and vent valves, that maybe used in association with the module 16. Furthermore, the modulecontrol unit 60 controls other devices 148 related to operation of thethermal control unit, including pumps and valves, that may be used tocontrol the temperature of the reactor 30 positioned in the module 16.

With reference again to FIG. 5, the user I/O units 62 receiveinstructions from the user of the modular reactor system related to anindividual module positioned in a slot of the backplane. The module I/Ounits also deliver outputs to the user of the modular reactor systemrelated to an individual module positioned in a slot of the backplane.To this end, the module I/O units 62 monitor and control various userinterfaces. For example, the module I/O units receive inputs related towhether a user has manually opened or closed one of the bubbler pathswitches 38. In addition, the module I/O units may be used to providewarnings related to particular modules, such as a warning lightindicating that the reactor in a particular module has reached acritical temperature and is overheating.

In the embodiment of FIG. 5, each module ID unit 22 is associated withone of the slots of the backplane 12. When a module is positioned in oneof the slots, the module ID unit 22 associated with that slot isoperable to read the electronic tag located on the module positioned inthe slot and thereby identify the specific module positioned in theslot. The module ID unit 22 then relays the identification of the moduleto the processor 54 and computer 18. Based on the particular module IDunit 22 that reports a reading, the computer can recognize a particularmodule in a particular slot of the backplane 12. This provides thesystem with the ability to distinguish one module over another module inany given slot, and thereby carry out specific instructions for thatmodule, regardless of the slot in which the module is placed.

Reactor Modules

With reference to FIGS. 7-9, each reactor module includes a module shell70 and a reactor 30 for holding reaction contents. The module shell 70is sturdy and typically comprised of steel or other metallic material.Of course other rigid materials could be used to form the module shell70. The module shell 70 includes two sidewalls 80 and a top handle 82bridging the two sidewalls. A reactor seat 72 holding a reactor 30 ispositioned between the two sidewalls 80. A reactor clamp 84 extendshorizontally from the top handle 82 so the clamp 84 is positioneddirectly above the reactor seat 72. A protective shield 85 is fastenedto the reactor clamp and extends to the reactor seat 72. The protectiveshield 85 is transparent and comprised of polycarbonate or othermaterial resistant to shattering. The protective shield 85 provides abarrier between an individual and the thermal fluid flowing through thereactor jacket, and thus provides a safety device that helps to block anindividual watching an experiment in the reactor 30 from escapingthermal fluid should the reactor 30 shatter. The backlight 25 in thehousing is positioned to shine through the reactor 30 and protectiveshield 85 to provide improved viewing of the reactor.

A module lip 81 is located along the base portion 83 of each sidewall80. Each module lip 81 is designed to interact with a rail 21 located inone of the slots 20 of the backplane 12, and thereby secure the modulein the slot of the backplane. As mentioned previously, the lip mayinclude a slotted rack designed to mesh with pinion gears on the siderails and thereby assist with smooth insertion of the module into theslot.

An instrument box 76 is positioned below and in front of the reactorseat 72, between the two sidewalls. The instrument box 76 carries twopumps 86, two gas fittings 88, and a pressure/vacuum fitting 89. Tworeagent seats 74 are located below and in the front of the instrumentbox 76. The reagent seats 74 are dimensioned to hold two bottles/vessels90 (see FIG. 2) containing reagents to be added to the reactor 30 duringthe experiment. The pumps 86 are used to transfer reagents in thereagent bottles 90 to the reactor 30. To accomplish this, tubes 31 (seeFIG. 2) are extended between each reagent bottle 90 and the pumps 86.Additional tubes 31 are extended from the pumps 86 to the reactor 30.Operation of one of the pumps 86 draws reagent from the reagent bottle90, through the pump 86 and into the reactor chamber 96 (see FIG. 10A).Tubes also extend from the gas fittings 88 to the reagent bottles 90and/or the reactor 30. The tubes connected to the gas fittings 88provide an inert gas to the reagents 90 and/or the reactor chamber 96.Furthermore, a tube (not shown) extends from the pressure/vacuum fitting89 to the reactor 30. This tube may be used to apply a pressure orvacuum to the reactor 30 during an experiment. Any number of flexiblelaboratory tubes and fittings known to those of skill in the art may beused to make the above-described connections.

The reactor 30 sits in the reactor seat 72 of the module shell and isheld securely to the module shell by reactor clamp 84. The reactor 30 istypically comprised of glass, or other material impervious to mostchemical reactions. As shown in FIG. 10A, the reactor 30 includes anexterior reactor wall 98 that surrounds an interior glass wall 95 toform a thermal control chamber 97 there between. The interior glass wall95 defines a reactor chamber 96 where reagents and other solutions areintroduced when conducting experiments in the reactor. A reactor mouth91 is located at the top of the reactor and leads to the reactor chamber96. A reactor lid 92, as shown in FIG. 22, is removably positioned ontop of the reactor mouth 91. An o-ring is placed upon the reactor mouth91 to facilitate sealing of the reactor lid 92 to the reactor mouth 91.A reactor junction is formed in the area where the reactor mouth 91seals to the reactor lid 92. As used herein, the term “reactor junction”is not limited to the portions of the reactor mouth 91 and reactor lid92 that physically seal, but also include portions of the reactor mouthand reactor lid immediately adjacent thereto, including externalportions of the reactor mouth and reactor lid that lead immediately tothe sealing portions.

Referring to FIGS. 22 and 23, the reactor lid 92 includes a number oflid ports 93 that provide access into the interior of the reactor. Thelid 92 includes a stirrer port 350 positioned at the top center of thereactor lid 92. The stirrer port 350 is designed to accept the stirrershaft 79 of a mechanical agitator in order to stir the contents of thereactor chamber 96. Peripheral ports 352, 354, 356, 358, 360 and 362,are each provided for additional access to the reactor chamber 96through the lid 92. These peripheral ports may be used to insert variouslaboratory instruments and feed lines into the reactor chamber. Forexample, the peripheral ports may be used to insert an automatedsampler, temperature probes, pH probes, inert gas feeds, and reagentfeeds into the reactor chamber. Peripheral ports 352, 360 and 362 aredesigned with a standard ChemThread® No. 12 thread pattern. Feed ports354 and 358 are each designed with a standard ChemThread® No. 4 threadpattern. Peripheral port 356 is designed with a standard taper “24/40”type female connector. As shown in FIG. 23, peripheral ports 352, 356,360 and 362 are all spaced 90° apart around stirrer port 350. Peripheralports 354 and 358 are each spaced 45° apart from peripheral port 356.

With reference again to FIG. 10A, the exterior glass wall 98 defines atemperature regulation chamber 97 with the reactor 30. The temperatureregulation chamber 97 may also be referred to herein as a “jacket” or a“cooling chamber”, but it is recognized that the chamber holds fluidthat may assist in cooling or heating the contents of the reactor. Aninlet port 100 and an outlet port 102 are provided in the exterior glasswall 98. The inlet port 100 and outlet port 102 each include a threadedportion 99. In addition, both the inlet port 100 and the outlet port 102have a “quick connect” attachment 101 positioned thereon. As usedherein, the term “quick connect attachment” or “quick connect connector”refers to a connection device that facilitates easy and secureconnection to an accompanying connector by simply inserting one quickconnect connector into an accompanying connector without the need fortightening, twisting or otherwise clamping or locking the connectorstogether. Plastic threaded sleeves 103 screw on to the threaded portionof inlet port 100 and outlet port 102 to secure the quick connects tothe ports 100 and 102. The quick connect attachments 101 on the reactor30 are designed to mate with complimentary quick connect connectorspositioned in the fluid ports 23 of the backplane.

With reference to FIG. 10B, quick connect attachments 101 include a baseelement 101 c. A shaft 101 d (also referred to herein as a “stud”) isattached to the base section 101 c. A first O-ring groove 101 a and asecond O-ring groove 101 b are circumscribed about shaft 101 d. O-rings101 f and 101 g, preferably made of an elastomeric compound, aredeposited into first O-ring groove 101 a and second O-ring groove 101 b,respectively. First O-ring groove 101 a and second O-ring groove 101 bpreferably accept the same size of O-ring. The base element 101 c has alarger external diameter than shaft 101 d. An opening (not shown)extends through the center of shaft 101 d and base element 101 c tocreate a channel through which fluid may flow.

Plastic sleeves 103 are open-ended, hollow cylinders which include firstopening 103 a, second opening 103 b, and sleeve threads 103 c. Incomparison to quick connect attachments 101, the diameter of firstopening 103 a is greater than the diameter of shaft 101 d, and smallerthan the diameter of base element 101 c. The diameter of second opening103 b is similar to the external diameter of inlet port 100 and outletport 102. Along the inside of plastic sleeves 103, starting at secondopening 103 b, are sleeve threads 103 c which are complimentary tothreads 99 of inlet port 100 and outlet port 102.

The quick connect attachment 101 is inserted into the second opening 103b of the plastic sleeve 103, shaft 101 d end first, such that the shaft101 d extends out of the first opening 103 a, but the base element 101 cremains inside the plastic sleeve 103. The second opening 103 b of theplastic sleeve 103 is then positioned near the inlet port 100 or theoutlet port 102, and the threads 99 are engaged with the sleeve threads103 c. The plastic sleeve 103 is rotated until the base element 101 c ofthe quick connect attachment 101 tightly abuts the end of the inlet port100 or the outlet port 103. A base O-ring 101 e, made of an elastomericmaterial, is placed between the base element 101 c and the inlet port100 or outlet port 102, to create a tighter seal between quick connectattachment 101 and inlet port 100 or outlet port 102. Attaching quickconnect attachments 101 to inlet port 100 and outlet port 102 with theuse of plastic sleeve 103 creates a rigid connection between the quickconnect attachments 101 and the ports 100 and 102. These rigidconnections are used to allow the ports 100 and 102 to quickly andeasily connect to fluid ports 23 on the backplane 12 when a module isplaced in a slot of the backplane. This connection allows for thermalregulation fluid to circulate within the cooling chamber 97, asdescribed in greater detail below.

FIG. 8 shows a reactor 30 installed into a module shell 70. A thermalcontrol system 14 (see FIGS. 10 c and 10 d) is connected to a backplane12. Fluid ports 23 are fixed to the backplane 12, and are connected tothe thermal control system 14. Fluid ports 23 are of a complimentarydesign to quick connect attachments 101, and include a cavity (notshown) designed to releasably engage the shaft 101 d of the quickconnect attachment 101. The O-rings 101 f and 101 g, positioned in theO-ring grooves 101 a and 101 b, provide a tight seal between quickconnect attachments 101 and fluid ports 23. When engaged with the fluidports 23, the quick connect attachments 101 allow fluid to circulatefrom the thermal control system 14, through the cooling chamber 97, andreturn to the thermal control system 14.

FIG. 9 shows a rear view of a reactor 30 installed into a module shell70. Quick connect attachments 101 are shown attached to inlet port 100and outlet port 102 with the use of plastic sleeves 103. Quick connectattachments 101 are shown disengaged from fluid ports 23.

As described above, the quick connect attachments 101 allow the inletport 100 and outlet port 102 to be quickly and easily connected to thefluid ports 23 in the backplane 12. Connection of the inlet and outletports to the fluid ports 23 of the backplane allow thermal control fluidto flow into and out of the cooling chamber 97, thereby controlling thetemperature of the contents of the reaction chamber 96. The reactionchamber 96 is dimensioned to a particular reaction volume in whichvarious experiments may be conducted. The reaction volume is typicallybetween 30 ml and 500 ml. Of course, greater reaction volumes arepossible, but as the reaction volumes increase, the size of the modulesmust also increase. The lower end of reaction volume is limited by anyminimum volume required to allow use of certain desired laboratoryinstruments, such as temperature probes, stirrers and sampling probes.For example, a particular temperature probe and stirrer combination mayrequire at least 50 ml of fluid in order for both instruments to operateproperly.

A stirrer 78 is also shown in FIG. 10A. The stirrer includes a shaft 79and propeller 77 used to stir the contents of the reactor 30 during anexperiment. Although the portion of the stirring shaft shown in FIG. 10Ais free floating within the reaction chamber 96, the stirring shaftactually extends from the reactor chamber 96 through a port 93 on thereactor lid 92. As shown in FIG. 4, a quick connect 136 connectiondevice is used to attach the stirrer shaft 79 to the drive shaft 134 ofthe motor 130 when the module holding the reactor is positioned withinone of the slots 20 of the backplane 12. Of course, the quick connect136 may take one of several different forms. For example, the quickconnect 136 may be a connecting shaft having one end that fits over thestirrer shaft 79 and another end that fits over the drive shaft 134 ofthe electric motor 130, thereby locking the drive shaft to the stirrershaft.

Referring again to FIG. 9, each reactor module 16 includes a back plate64 having an electrical connector 65 and a gas line connector 66positioned thereon. The electrical connector 65 mates with one of theelectrical connectors 40 in the backplane 12 when the module 16 isplaced in one of the slots 20. Likewise, the gas line connector 66 mateswith one of the gas line connectors in the backplane 12 when the module16 is placed in one of the slots 20. In this manner, when a module 16 isplaced in the slot 20, the module is powered through the backplane 12and is in electronic communication with one of the control modules ofthe backplane. Furthermore, a gas pressure and a vacuum source is madeavailable to the module 16 through the gas line connector 66.

An identification in the form of an electronic tag is held by the backplate 64 of the module shell 70. Electronic tags are well known to thoseof skill in the electrical arts, and are available from a number ofcommercial sources. As discussed previously, an identification reader 22is located above each slot of the backplane. When a module 16 is placedin a slot 20 of the backplane, the reader 22 is aligned with theelectronic tag held by the back plate 64, allowing the reader toidentify the module and distinguish it from other modules in other slotsof the backplane 12. Although the electronic tag is not shown in FIG. 9,the electronic tag is retained below the surface of the back plate 64 atthe location shown by reference number 63, between the electricalconnector 65 and gas line connector 66. In this embodiment, theelectronic tag is a radio frequency identification (RFID) tag, allowingthe tag to be read by the electronic tag reader without actuallycontacting the tag. The electronic tag could also be mounted on thesurface of the back plate 64 or on any other module location that allowsfor reading by the tag reader 22. Of course, other types of tags andreaders may be used, including optical tags such as bar codes. Otherexamples of identification that could be used include, withoutlimitation, infrared beacons, mechanical flags, and optical block codes.As another example, the identification could be an electronicidentification code magnetically or optically stored in a storage deviceretained on the module, and the identification reader could be a circuitor microprocessor that retrieves the stored code through the electricconnector on the module.

Each reactor module 16 is designed for repeated insertion into andremoval from any of the slots 20 of the backplane 12. When this happens,some connections between the module and the backplane occurautomatically, while other connections must be made manually. Forexample, as discussed above, proper insertion of a module into a slotwill cause the electrical connectors in the module and the backplane toautomatically mate. Likewise, proper insertion of a module into a slotwill cause the gas line connectors in the module and the backplane toautomatically mate. Furthermore, quick connects 101 will cause the inletport 100 and outlet port 102 of the reactor to be joined to the fluidports on the backplane. However, once a reactor module 16 is properlyseated in a slot of the backplane 16, the stirring shaft 79 must bemanually connected to the drive shaft 134 of the motor 130 using thequick connect coupler 136. Furthermore, the leads of temperature probes140 may be easily connected to the receptacles 44 dedicated totemperature measurements by plugging the leads into the receptacles.Likewise, the leads of pH probes 144 and other probes may be easilyconnected to the receptacle 44 dedicated to that particular measurement.

Thermal Control Unit

Once a module 16 is seated in a slot 20 of the backplane 12, one of thereactor thermal control systems 13 may be used to pump heating orcooling fluid (i.e. thermal control fluid) to the associated reactor 30through the quick connect 101 of the reactor. After reaching thereactor, the thermal control fluid flows in the thermal control chamber97 of the reactor between the interior glass wall 95 and the exteriorglass wall 98 and thereby heats or cools the contents of the reactionchamber, depending upon the temperature of the fluid and the reactionchamber.

In known systems, each reactor may be provided with a dedicated heatingelement so as to maintain the reactor at or above ambient temperature.In such a system, it is possible to heat various reactors to differenttemperatures. Some systems further provide a single source of coolingfluid to the entire array of reactors for maintaining temperature of allof the reactors below ambient temperature. When conducting the sameprocess on all reactors in a device, this may be useful. However, theseknown systems do not allow sufficient flexibility for the module reactorsystem of the present invention.

Accordingly, one aspect of the present invention comprises a thermalcontrol system which allows individual reactors to be maintained at adesired temperature regardless of ambient temperature or the temperatureat which other reactors are maintained. Referring to FIG. 10C, oneembodiment of the thermal control system of the present invention isdescribed.

FIG. 10C shows the one of the individual reactor thermal control systems13. Reactor thermal control system 13 comprises a valve 164 and athermal control fluid reservoir 166. Heat exchanger 168 and heat element170 are located within thermal control fluid reservoir 166. Thermalcontrol fluid pump 172 takes a suction on thermal control fluidreservoir 166 to pump thermal control fluid through supply line 174.After passing through thermal control chamber 97, thermal control fluidis returned to reservoir 166 by return line 176. Thermocouples 178 and180 may be provided on supply line 174 and return line 176. Fluid ports23 are provided on supply line 174 and return line 176. According tothis embodiment, fluid ports 23 are designed to automatically engagewith quick connects 101 when module 16 is seated in a slot 20 of thebackplane 12. Relief valve 182 is provided to maintain a safe pressurein the thermal control fluid reservoir 166 even with expansion andcontraction of the thermal control fluid over a range of temperatures.

Cooling for the system in this embodiment is provided by a chill fluidsystem which is described in reference to FIG. 10D. Thermal controlsystem 14 comprises chill fluid supply system 184 which includes chillfluid reservoir 186, supply manifold 188 and return manifold 190. Chillfluid pump 192 takes a suction on chill fluid reservoir 186 and supplieschill fluid to supply manifold 188. Back pressure control valve 194maintains the pressure of supply manifold 188 even as the heat load onthe system changes, as will be discussed further below. Chill fluidsupply manifold 188 provides chill fluid to individual reactor chillfluid systems by chill fluid supply lines 196. Fluid is returned fromthe reactors by chill fluid return lines 198. In this embodiment, valve164 is located on the supply line of the reactor chill fluid system,however, it may alternatively be located on the return line.

In operation, thermal control fluid pump 172 takes a suction on thermalcontrol fluid reservoir 166 to constantly pump thermal control fluidthrough supply line 174. Of course, temperature control software may beused to vary the speed of thermal control fluid pump 172 or even tocontrol thermal control fluid pump 172 on and off in response to sensedconditions or a recipe if desired. Temperature control software may alsobe used to control heat element 170 as necessary to provide heat tothermal control fluid reservoir 166. Chill fluid to thermal controlfluid reservoir 166 is provided by positioning valve 164. This regulatesthe amount of chill fluid that passes through heat exchanger 168 andcools the thermal control fluid in thermal control fluid reservoir 166.

According to one embodiment, control of valve 164 is effected bytemperature control software. Chill fluid flow is controlled by valve164 since supply manifold 188 of chill fluid supply system 184 ismaintained at a positive pressure by back pressure control valve 194 andchill fluid pump 192. Specifically, as a valve throttles opens, thepressure in supply manifold 188 will tend to drop. However, backpressure control valve 20 will throttle shut so as to maintain positivepressure within supply manifold 188, thus assuring a supply of chillfluid to other reactors. Alternatively, a variable speed chill fluidpump may be used to increase supply of chill fluid as a valve throttlesopen. According to one embodiment, the system is sized such that thepressure within the supply header is maintained at a constant pressureregardless of whether all the valves are full open or full shut.

In accordance with the embodiment of the invention disclosed in FIGS.10C and 10D, thermocouples 178 and 180 may be monitored by temperaturecontrol software and used as input to control the heater and supply ofchill fluid. Additional inputs to the temperature control software whichmay be used include position of the valves, chill fluid pump speed orchill fluid flow, back pressure valve position, chill fluid supplymanifold pressure, pressure and temperature of the reactor vessel, andtime.

Those of skill in the art will recognize that although one embodiment ofthe thermal control system of the present invention is described above,the present invention encompasses a number of alternative embodiments.By way of example, but not of limitation, the thermal control system ofthe present invention may be used with a single reactor vessel or withan array of more than the four shown in FIG. 10D. Additionally, althoughcooling is provided in the embodiment discussed by chill fluid, anyacceptable cooling medium may be used, and the term “chill fluid” asused herein refers to any such acceptable cooling medium. Moreover, thethermal control system need not be automatically connected when a module16 is placed in a slot 20 of the backplane 12.

Reactor Clamp

In order to facilitate a safe operating environment, a reactor 30 and areactor lid 92 should, in a preferred embodiment, be securely fastenedto a structural framework while a reaction is run inside the reactor 30.With reference to FIGS. 8 and 16-21, a clamp 84 is releasably attachedto module shell 70 using clamp attachments 308, which include posts thatjoin with holes 75 in the module sidewalls 80 to secure the clamp to themodule shell 70. In operation, the clamp 84 contacts portions of thereactor junction, including portions of the reactor mouth 91 and thereactor lid 92. The clamp 84 is operable to release the reactor lid 92from the reactor 30 when the pressure within the sealed reactor chamber96 (formed by the union of reactor 30 and reactor lid 92) reaches athreshold pressure. The term threshold pressure, as used herein refersto the pressure in the reactor chamber 96 required apply sufficientforce to the clamp to temporarily release the reactor lid from thereactor mouth, when the clamp is being used to hold the reactor lid tothe reactor mouth.

FIG. 16 shows a bottom view of clamp 84. The clamp 84 includes a firstor front clamp member 304 releasably joined to a second or rear clampmember 306. Retaining bolts 302 extend through bores (not shown) in thefront clamp member 304 and into channels 314 in the rear clamp member306. Each of the retaining bolts 302 includes a knob 300 on the end ofthe retaining bolts 302 extending from the front clamp member 304.Retaining bolts 302 can include a bar, stud, rod, or other elongatedmember extending between front clamp member 304 and rear clamp member306. Nuts 310 a and 310 b are recessed in the channels 314 of the rearclamp member 306. A spring 312 is retained upon the retaining bolts 302between nuts 310 a and 310 b in each channel 314 The retaining bolts 302extend through the front clamp member 304 and into rear clamp member306, where retaining bolts 302 also extend through nut 310 a. Theretaining bolts 302 extend through the springs 312 in the channels 314.Threads on the retaining bolts 302 engage complimentary threads (notshown) on nuts 310 b. Nuts 310 a do not include threads. Thus, when theretaining bolts 302 are rotated, nuts 310 a remain stationary, but nuts310 b travel along the channels thereby compressing or relaxing springs312, as the case may be. The more the springs compress in the channel,the more force is required to separate the front clamp member 304 fromthe rear clamp member 306. Accordingly, knobs 300 and retaining bolts302 comprise an adjusting means, for purposes of adjusting tension insprings 312 and the force holding the first clamp member 304 to thesecond clamp member 306.

As shown in FIGS. 10A and 20-22, the mouth of the reactor 91 and thebottom of the reactor lid 92 are angled outwardly. As shown in FIGS. 17and 18, and further illustrated in FIG. 19, an angled edge 322 isinscribed along the inside of the front clamp member 304 and the rearclamp member 306 such that the angled edge 322 is continuous when frontclamp member 304 and rear clamp member 306 are joined together. Anglededge 322 includes top angled edge 316 and bottom angled edge 318.Additionally, O-ring grooves 320 are inscribed along top angled edge 316and bottom angled edge 318. O-rings or partial O-rings (not shown) aredeposited into O-ring grooves 320 to assist in providing a cushionedsurfaces for contacting the reactor junction and holding the reactor lid92 to the reactor mouth 91.

When the front clamp member 304 and rear clamp member 306 are joined,and the knobs 300 are tightened, the threads (not shown) on retainingbolts 302 operate on complimentary threads (not shown) on nut 310 b suchthat nut 310 b moves closer to nut 310 a. The springs 312 between nuts310 a and 310 b are compressed by the movement of nuts 310 b. Thecompression of the springs 312 serves to impart a force which biases theknob ends of the bolts toward the channels 314 of the rear clamp member306. This causes the knobs 300 to press against the front clamp member,or the shield 85, if shield 85 is installed, and bias the front clampmember 304 toward rear clamp member 306, thereby tightly joining thefront clamp member to the rear clamp member. When the clamp is installedon the reactor junction, the angled edge 322 inside the clamp 84 forcesthe reactor 30 and the reactor lid 92 together tightly by top anglededge 316 (or a surface associated therewith, such as an O-ring) pressingdown against the outwardly angled bottom of the reactor lid 92, andbottom angled edge 318 (or a surface associated therewith, such as anO-ring) pressing up against the outwardly angled top of the reactor 30(i.e., the reactor mouth 91). FIG. 20 shows an exploded, cut-away viewof the reactor 30 and the reactor lid 92 pressed together by top anglededge 316 and bottom angled edge 318. An o-ring 317 is shown positionedbetween the reactor lid 92 and the reactor mouth 91. As the springs arefurther compressed, the forces acting against the reactor lid and thereactor mouth increase. Alternative means for biasing front clamp member304 against rear clamp member 306 (and thereby creating forces biasingthe reactor lid 92 to the reactor mouth 91) include using an elastomericband or string, a gas or liquid pressure apparatus, or a flexible metalapparatus.

Referring again to FIG. 7, clamp 84 is attached to module shell 70, andthe clamp 84 is also attached to reactor lid 92 and reactor 30. ReactorO-ring grooves (not shown) are inscribed about the top of the reactor 30and the bottom of the reactor lid 92. The union of the reactor 30 andthe reactor lid 92, along with the inclusion of an elastomeric O-ring(not shown) into the reactor O-ring grooves 320 creates a sealed reactorchamber 96. When the reactor lid 92 and the reactor 30 are attached tothe clamp 84, and knobs 300 are tightened, the angled edges 322 of theclamp 84, as shown in FIG. 10 d, ensure that the reactor lid 92 and thereactor 30 are sealably engaged as long as the pressure within thereactor vessel remains below some threshold pressure. Under reactionconditions inside the reactor chamber 96, a reaction may evolve a gas,which creates a pressure inside the reactor chamber 96 greater than thepressure of the surrounding atmosphere. Under high pressure inside thereactor 30, gas pressure pushes the reactor lid 92 away from the reactor30. Under this high pressure, the reactor lid 92 applies a force to thetop angled edge 316, and the reactor 30 applies a force to the bottomangled edge 318. The vertical separation force imparted by the reactor30 and the reactor lid 92 is converted into a horizontal force by topangled edge 316 and bottom angled edge 318. At a threshold internalreaction chamber pressure, this applied horizontal force causes thesprings 312 inside the clamp 84 to contract further, which allows frontclamp member 304 to slightly separate from rear clamp member 306. Thedisengaging of front clamp member 304 from rear clamp member 306 allowsthe reactor lid 92 and the reactor 30 to separate slightly, while stillbeing retained by top angled edge 316 and bottom angled edge 318,respectively. FIG. 21 illustrates an exploded, cut-away view of reactorlid 92 and reactor 30 separating, while still being retained by topangled edge 316 and bottom angled edge 318, respectively. The slightseparation of the reactor lid 92 from the reactor 30 serves to ventexcess pressure from the internal reaction chamber 96 to the surroundingatmosphere through the openings created by the separation of front clampmember 304 and rear clamp member 306, and return the reactor 30 to asafe operating pressure. When a safe operating pressure inside thereactor 30 is reached, the springs 312 expand, which forces the frontclamp member 304 and the rear clamp member 306 together, which in turncauses top angled edge 316 and bottom angled edge 318 to exert increasedpressure on reactor lid 92 and reactor 30, to seal the reactor lid 92 tothe reactor 30. The reversibility of this pressure venting processallows reactor 30 and reactor lid 92 to be separated and rejoinedmultiple times during the course of a reaction without operatorintervention, should reaction conditions require.

Computer Software

The computer 18 includes software that an automated laboratoryworkstation used to control the laboratory instruments and/or planautomated experiments using the modular reactor system 10. The computer18 includes a microprocessor/controller running an operating system suchas WINDOWS® 2000 that allows for graphical program manipulation. Aninput/output device is connected to the microprocessor and allows theuser of the modular reactor system 10 to interact with themicroprocessor. The input/output device typically includes a keyboard,monitor, mouse, speakers and/or other input/output devices used inassociation with computers such as microphones, touch screens,trackballs, etc. As shown in FIG. 5, the microprocessor is connected tothe processor 54 of the backplane 12 through RS-232 interface 51. Theprocessor 54 interacts with the microprocessor of the computer and thededicated module control units 60 to deliver control signals to thelaboratory devices associated with the modules 16. The laboratorydevices 118 may include, for example, pumps, stirrers, heaters, coolers,vacuum devices, temperature monitors, pressure monitors, and othersensors and laboratory instruments. Furthermore, the terms “laboratorydevices” or “laboratory instruments” as used herein may refer to anynumber of devices used in chemical processes, regardless of size, andregardless of whether the device is or can be used in a traditional“laboratory” setting.

With reference to FIGS. 11A and 11B, the software stored in the computer18 provides a graphical user desktop 232 for controlling and/orprogramming the laboratory devices, including the laboratory deviceslocated on any module positioned in any seat 20 of the backplane 12. Thegraphical user desktop 232 may be accessed by the user of the modularreactor system through the input/output device. As shown in FIG. 11A,the graphical user desktop 232 includes an overview screen 234 thatdisplays graphical representations of each module reactor 230. In theembodiment shown, the overview screen 234 is divided into four quadrants239, with each quadrant showing one module reactor 230. At thediscretion of the user, the modules may be viewed or may remain hiddenin each quadrant. When a module reactor is displayed in one of thequadrants 239, a representation of the reactor 230 is shown along with atable of data 231 specific to that module reactor. A menu 233 is alsoprovided next to each reactor 230, thus providing the user with optionsconcerning control of the module and the data shown in association withthe module.

One of the menu 233 options allows the user to provide configurationparameters for the particular module to the computer. In particular, byselecting the “configure module” option from the menu 233, the user isprovided with a configuration screen, such as that shown in FIG. 15. Theconfiguration screen 291 provides a name block 292 for the user toinput/edit the module name that will be associated with theconfiguration. In addition, the configuration screen allows the user toinput the reactor size associated with the module in block 294,calibrate the feed pumps associated with the module in block 296, andinput a number of alarm settings in block 298. After selecting the “OK”button on the configuration screen, the user is returned to the overviewscreen.

Referring again to FIG. 11A, the menu 233 also provides the user withthe ability to remove the module from the screen by selecting the“Remove Module” option from the menu. As explained in more detail below,the menu 233 also provides the user with options related to a program or“recipe” Furthermore, the menu provides the user with the ability torecord a series of steps that are taken with respect to a particularmodule and save those steps in a “recipe”. This process of recording isdescribed in further detail in pending U.S. application Ser. No.10/162,272, which is incorporated herein by reference.

A larger, more detailed overview screen for each reactor 230 may beviewed by clicking on the quadrant number 257 or the module name 202associated with the reactor 230 shown on the overview screen 234. Oneembodiment of the more detailed overview screen 237 is shown in FIG.11B. As shown in FIG. 11B, the more detailed overview screen 237 issimilar to the overview screen 234 shown in FIG. 11A, but includesadditional information. The more detailed overview screen 237 includes arepresentation of the reactor 230 located on the module, a menu 249, anda table of data 248 for each reactor. The table of data 248 includescolumns showing the target and actual amounts for various parametersrelated to the reactor, including temperature of the reactor,temperature of the jacket, feed volumes for the reagents, stirrer speedand torque, pressure within the reactor and pH within the reactor. Athird column of feed rates is also provided for determining the rate atwhich reagents will be fed to the reactor. The overview screen 237 alsoincludes a graph that provides a visual display of selected parametersshown in the table 248 during a chosen time period. The more detailedoverview screen 237 also includes representations of the reagent feeds240 and 242, a representation of the vacuum line 255 and representationof the inert gas/pressure line 253.

With continued reference to FIGS. 11A and 11B, the graphical userdesktop 232 allows the user to easily control and monitor the progressof an experiment from the overview screen 234. The particular reactorbeing shown on the overview screen is identified by a reactoridentification block 200. The reactor identification block 200 shows thename 202 of the module holding the reactor. Although the modules areformally identified by the modular reactor system based on theelectronic tag on the module, the graphical user desktop allows the userto identify modules by more user-friendly names. As shown in FIG. 11B,the module holding the reactor represented by reference numeral 230 isnamed “Jim 001”. If the user wishes to see the set-up for a reactorassociated with a different module, the user simply goes to overviewscreen 234 and selects the module. The detailed view of that module maythen be displayed on the full screen, as described above.

The graphical user desktop 232 also provides the user with the abilityto control each of the laboratory devices used in the experimentdirectly from the screen. Accordingly, the modular reactor system 10allows the user to conduct an experiment by commanding one instrumentafter another to take certain actions, thereby orchestrating theexperiment step-by-step, in real-time, from the desktop 232.Alternatively, as explained in more detail below, the user may programthe system to run independent of human operation, and thereby leave thedesktop while the experiment is automatically carried out under computercontrol.

Real Time Experiment Control

All laboratory devices depicted on the graphical user desktop 232 may becontrolled by clicking on the control “button” (i.e., selectable option)associated with that device (e.g., the “Feed A Control” button 241, the“Feed B Control” button 243, the “Stirrer Control” button 245, or the“Temperature Control” button 247). A mouse or other input device isprovided to allow the user to select the desired device/buttons formanipulation. For example, if the user selects the “Stirrer Control”button 245, a dialog box will be displayed showing the stirrerparameters, as shown in FIG. 12. Thus, if the user wants to change thestirrer speed from 550 rpm to 500 rpm, the user selects the display ofthe stirrer setpoint rpm in the dialog box and, using the keyboard,inserts the number “500” in place of the number “550.” Next, the userselects the “Accept” button at the bottom of the dialog box, and thestirrer immediately starts spinning at the new rate of 500 rpm. Ofcourse, any number of different means may be used to allow the user toenter operating parameters and the system to receive such parametersrelated to a particular laboratory device. For example, representativedevice control panels could be used to allow the user to enter theoperational parameters or graphical parameter representations could beused to adjust parameters (e.g., clicking on a representative stirrercould adjust the stirrer spin speed). As a further example, operationalparameters could be keyed into the system, adjusted by a click of themouse, or entered vocally.

Similarly, the user may click on one of the “Feed Control” 241 or 243buttons to control the feed rate and amount of liquid product to be fedto the reactor. After clicking on the “Feed Control” buttons, a dialogbox appears, similar to that shown in FIG. 12, allowing the user toinsert a desired feed rate (in weight or volume per minute) and adesired feed amount (in total weight or volume). Again, after clickingthe “Accept” button at the bottom of the dialog box, the workstationwill begin the desired feed.

The desktop also provides for temperature control of the reactor. Afterclicking on the “Temperature Control” button 247, a dialog box appears,allowing the user to choose the desired temperature measurement tocontrol. After choosing a desired temperature or temperature range, theuser also provides a ramp rate which defines the rate at which thetemperature will change (e.g., ° C./min). After completing theinformation in the dialog box, the user clicks the “Accept” button atthe bottom of the dialog box and the workstation immediately begins tocontrol the identified temperature based upon the users instructions.When the temperature control determines that the temperature is not inthe preferred range, heat transfer into or out of the reactor iscontrolled as described above with respect to the thermal control unit14.

With reference to FIG. 11B, the information presented on the overviewscreen 237 continuously changes based upon actual experiment conditions.For example, the “Feed A” data box 290 is periodically updated to showthe actual amount of fluid that has been fed through the Feed 1 pump.Likewise, other cells of the “Reactor Conditions” table 248 keep trackof various temperatures, reactor pressure and reactor pH. Also, the“Reactor Contents” data box 298 keeps track of the total volume of fluidin the reactor, if applicable. If any experiment parameter reaches acertain threshold, a warning will be sounded or displayed on thedesktop. For example, if the volume of reactor contents becomesdangerously high, an alarm sounds or a message appears on the screenwarning the user to avoid over-filling the reactor. Similarly, if thereactor contents reach a threshold temperature, making the reactorunstable, a warning will be sounded or displayed, warning the user todecrease the temperature of the reactor contents.

Recipe Programming and Unattended Operation

If the user desires, the system 10 may be pre-programmed to complete allsteps of an experiment automatically with respect to a particularmodule, thereby allowing the experiment to be conducted unattended oncethe module is positioned in a slot 20 of the backplane 12. By clickingon the “Edit Single Recipe” button from the menu 233 or 249, or byselecting the “Recipe Maintenance” option 256 provided along the top ofthe overview screen, the user is presented with a “recipe editor” 258,such as that shown in FIG. 13. The recipe editor 258 is a tool forprogramming an experiment to be performed automatically by defining a“recipe” (i.e., a series of steps to be followed to accomplish a desiredresult). The recipe is saved as an executable computer program that canbe played using the system software. The recipe editor includes a “StageDetails” tab 262, a “Stage Specials” tab 264, and a “Stage Overview” tab268. Each tab provides different options to the user concerning therecipe.

Under the “Stage Details” tab 262, the recipe editor 258 is designed toset up the automated experiment to be conducted in the reactor of aparticular module as a series of steps or stages. A stage indicator 260is provided on each screen of the recipe editor on the top right of thescreen. The stage indicator shows an indication of the stage as well asarrows for maneuvering between stages. The user programs each stage ofthe recipe under the “Stage Details” tab, and by using the stageindicator to maneuver between stages. Each screen under the “StageDetails” tab includes a variety of icons representative of variousoperations (e.g., temperature control 270, addition of liquids 272,valve settings 274, pressure control 278, stirring 276, etc.). The useridentifies a desired action in each stage by inputting performanceinformation in the boxes associated with each icon. For example, if theuser wants to start the experiment by setting the reactor temperature to25° C. for at least 20 minutes, the temperature set point of 25° C. isindicated in temperature mode box 270 and a hold time of 20 minutes isindicated in the hold time box 280. After identifying this first stage,the user then moves to the next stage by pressing the “>” arrow in thestage indicator 260. In the next stage, the user programs an additionalstep to be carried out, such as adding a new chemical through the“addition mode” box 272 or stirring the reaction through the “stirrer”box 276. When additional stages are added, the total number of stages inthe experiment are shown in the stage indicator 260. For example, inFIG. 13, a seven stage experiment has been created and the first stageof the experiment is displayed in under the “Stage Details” tab. Theuser can move between stages by clicking the arrows to the right andleft of the indicated stage in the stage indicator 260. By movingthrough the experiment stage-by-stage, the user defines the completeexperiment, breaking down the experiment to define how the equipment andlaboratory devices should function in each stage.

In addition to automated stages, the user may program a manual stage.This is done by clicking the “enabled” button in the manual confirmationbox 282, and inserting instructions on the manual step to be taken bythe user. This feature is especially useful when solid or liquidreagents are to be added to the reactor during an experiment. Forexample, if 10 ml of NaCl is to be added to the reactor in a givenstage, the user can note this as a stage in the recipe editor and notethat manual confirmation is required before moving to the next stage.Thus, when the workstation automatically replays the recipe, aconfirmation box will appear asking if 10 ml of NaCl has been added tothe reactor. The confirmation box will include “yes” and “no” buttonsthe user may click in response. The workstation will not proceed withthe experiment until the user makes a positive response that the NaClhas been added. Of course, the recipe programmer must recognize thatmanual confirmation steps can not be used if he/she desires to conduct afully automated experiment with no user present to oversee theexperiment.

The “Stage Specials” tab 264 allows the user to customize certainfunctions associated with different stages of the programmed experiment.For example, the “Stage Specials” tab provides for experimenttermination conditions (e.g., excessive pressure, temperature, etc.),data logging rates (i.e., snapshot of experiment conditions taken at aperiodic rate), and special alarm settings (e.g., excessive pressure,temperature, etc.).

The “Stages Overview” tab 268 allows the user to review the entireexperiment in a single spreadsheet format, such as that shown in FIG.14. The “Stages Overview” tab 268 allows the user to see stages next toeach other in tabular fashion, allowing the user to view the entireexperiment on a single page, line-by-line. If the user sees any problemswith the experiment set-up or desires changes in any particular stage,he or she can double click on the line showing the particular stage andbe transferred to the “Stage Details” tab for that stage. At the “StageDetails” tab, the user may make any required modifications to theexperimental set-up. Alternatively, the user may make modifications todifferent stages directly from the “Stages Overview” tab 268 by singleclicking on an particular information item and changing the entry forthat item. For example, if the user wants to change the hold time instep one from 20 to 25 minutes, the user can click on the “20” in lineone and enter the new data in place of the old.

After all stages of a recipe are entered into the system, the recipe issaved by clicking the “Save” button 284. Thereafter, the created recipeis saved and the user is returned to the overview screen 234 or 237.

At the overview screen 234 or 237, the user may execute the recipe byclicking on the “Execute Recipe” button from the menu 233 or 249.Choosing this “Execute Recipe” button will allow the user to choose froma list of recipes saved in the system. After the user chooses a recipe,the software will confirm that all laboratory devices required toexecute the chosen recipe are connected to the system. If all requiredlaboratory devices are not connected, the user will receive an errormessage informing the user that the required devices to execute therecipe are not properly connected. Also, before starting the experiment,the system will request confirmation that the reactor 30 has been filledwith any required starting materials. Finally, before starting theexperiment, the system will ask the user when he or she wants theexperiment to begin. The user generally has the ability to start theexperiment immediately or at a pre-defined time. For example, if theuser wants an experiment to start in the middle of the night, the usercan instruct the workstation to start the experiment at that time.

The overview screen 234 or 237 also provides the user with the abilityto edit any recipes saved in the system. This option is available byclicking the “Edit Single Recipe” button provided on the menu 233 or249. By clicking the “Edit Single Recipe” button, the user is presentedwith a list of recipes saved in the system. After the user chooses arecipe, the recipe information is presented in the recipe editor and therecipe may be edited in the recipe editor, as described above.

Operation of the Modular Reactor System

As discussed above, when a chemist wants to conduct an experiment in oneof the reactors, the experiment may be conducted in real-time orprogrammed into the computer for future automatic execution using themodular reactor system. It is anticipated that experiments using themodular reactor system will typically be pre-programmed for laterexecution. In particular, the modular reactor system allows a pluralityof chemists to each have control over a plurality of modules. Using thecomputer 18, each chemist may then program experiments to be conductedin each of the modules. As discussed above, because the modular reactorsystem is capable of taking different actions with respect to differentmodules in different slots of the backplane, the experiments programmedfor different modules may vary significantly in terms of functions usedin each experiment and steps conducted to complete each experiment. Forexample, one experiment may call for continuous stirring while anotherexperiment conducted in an adjacent module may call for no stirring. Asanother example, controlling the temperature in one module reactor mayrequire cooling fluid to flow into the cooling chamber at 5° C., whilecooling fluid for another module reactor in an adjacent slot may onlyrequire cooling fluid at 50° C.

After the module is set up to conduct the experiment as programmed, themodule is given to a laboratory technician for execution of theexperiments using the modular reactor system. The laboratory technicianplaces modules 16 in the backplane 12 as the slots 20 become available.When a particular module 16 is placed in the backplane, theidentification reader 22 reads the identification of the module 16 andforwards the identification to the processor 54 and computer 18. Thecomputer automatically recognizes the module and temporarily associatesthe module with the particular slot in which it was placed. The computeralso accesses the program associated with that module and determines ifthe module contains all laboratory instruments required to conduct theexperiment as programmed. Thereafter, when executing the instructionscontained in the program associated with that module, the computer usesthe laboratory instruments associated with the slot retaining the moduleto execute the instructions and thereby conduct an experiment in themodule reactor. In this manner, experiments may be programmed forindividual modules without limiting the module to any particular slot ofthe backplane.

A chemist wishing to use the modular reactor system first visits thecomputer 18 and, using the recipe editor, enters step-by-stepinstructions for completion of an experiment to be conducted in aparticular module. Part of the programming process involves associationof the planned experiment with one of the reactor modules. This may beaccomplished because each reactor module has a unique ID in the form ofa number, bar code or other identifier, allowing the chemist to identifythe reactor module to the computer. Of course, as discussed above,user-friendly names may be assigned to each module to help the chemisteasily remember the names of the modules. After programming a set ofinstructions for completing an experiment in a particular module, thechemist prepares the module and associated reactor for the automatedexperiment by inserting initial reaction contents into the reactorvessel, providing reagents to be added during the experiment in areagent bottle, attaching laboratory instruments to the reactor (e.g.,temperature sensors), attaching required tubes and lines on the module,and/or taking any other required preparatory steps. After the reactormodule is readied for the experiment, the chemist indicates that themodule is ready for an experiment in the backplane. This can beaccomplished by any of various protocols, such as placing the module ina queue or otherwise passing the module on to a laboratory technicianresponsible for keeping experiments running in the backplane. When aslot becomes available in the backplane, the laboratory technician seatsthe module in the open slot, making sure that all standard connectionsare made between the module and the backplane, including connection ofthe electrical connectors, gas line connectors and fluid ports. Thelaboratory technician also makes any additional required connectionsbetween the backplane and the module, such as connection of sensors toreceptacles 44 and connection of the stirrer shaft to the drive shaft ofthe motor.

When the backplane receives a reactor module, the identification on themodule allows the module to be associated with a pre-recorded recipe, ifapplicable. Thus, if the identification is a human readableidentification, the laboratory technician will indicate that theparticular module is seated in a particular slot. This allows thecomputer to retrieve instructions for that module and direct actions forthat module to the slot where the module is located. On the other hand,if the identification is an electronic tag or other machine-readableidentification, the tag reader reads the tag on the module and reportsthe identification of the module to the computer. Based on theidentification and the tag reader relaying the identification, thecomputer automatically recognizes the particular reactor module and theparticular slot of the backplane where the module is seated. Thecomputer then retrieves the instructions related to that particularmodule and proceeds to conduct the experiment designed for the materialsin the designated module, using the laboratory instruments on the moduleand associated with the slot in which the module was placed.Accordingly, the lab technician is not restricted to placing the modulein any particular slot of the backplane, as the computer has the abilityto recognize the module and execute specific instructions for themodule, regardless of the slot in which the module is placed.

Based on the information provided to the computer, the software residingon the computer 18 delivers control signals to the backplane, reactormodules seated in slots of the backplane, and the thermal control unit.These control signals allow experiments to be automatically conducted ineach reactor. For example, a control signal from the computer willinstruct a motor in the backplane to stir the contents of one of thereactors at a particular time, or instruct the thermal control unit todeliver liquid cooling agent to the reactor at a given time. Of course,the backplane is designed to accommodate a number of reactor modules, sonumerous experiments may be conducted simultaneously using the presentinvention. Furthermore, because of the modular nature of the system, themodular reactor system can simultaneously conduct a number of distinctexperiments. These distinct experiments may vary in any number ofdifferent ways, including distinct functions and processes, since thelaboratory instruments and tools available to each slot and the moduleplaced in that slot may be controlled completely independent of thelaboratory instruments and tools available to adjacent slots and modulesplaced in those slots. The computer is also capable of avoidingscheduling conflicts between various devices (e.g., conflicts with useof the robotic arm). However, scheduling conflicts will not typically bea problem, as each slot of the backplane typically has identicallaboratory instruments, and there are few, if any, laboratoryinstruments that must be shared between slots. The fact that each slotincludes a standardized set of laboratory instruments, allows any givenexperiment to be conducted in any given slot. Because the modularreactor system allows the chemist to pre-program experiments inindividual modules for later execution, and because the experiments maybe conducted automatically without the presence of the chemist, thechemist is freed to work on other tasks. For example, the chemist mayspend his or her time planning future experiments while otherexperiments are conducted automatically. Alternatively, the chemist mayqueue up a number of modules to for experiments during the night hours,when the chemist is away from the laboratory.

Although the present invention has been described in considerable detailwith reference to certain preferred versions thereof, other versions arepossible. For example, the physical form of the backplane and modulesmay take on number of different embodiments other than those described.In particular, the connectors and receptacles of the backplane could allbe positioned differently, or the top canopy could be removed from thebackplane. In addition, certain laboratory instruments could be added orremoved from the backplane or any of the modules. The modules could takeon different shapes or sizes, and different mechanisms could be used toseat the modules in the backplane. Furthermore, the graphical userdesktop used to conduct experiments could be set up differently thanthat shown and described. Therefore, the spirit and scope of theappended claims should not be limited to the description of thepreferred versions contained herein.

1. A modular reactor system comprising, a support housing having aplurality of module seats, wherein each module seat releasably engages areactor module having a reactor vessel coupled to a shell; a movablemotor coupled to the support housing, and a motor shaft operablyconnected to the motor such that when the motor is energized, the motorshaft rotates.
 2. The modular reactor system of claim 1, wherein themovable motor is connected to a gimbal.
 3. The modular reactor system ofclaim 2, wherein the gimbal is mounted on the support housing of themodular reactor system.
 4. The modular reactor system of claim 1,wherein the movable motor is movable by rotation about two differentaxes.
 5. The modular reactor system of claim 1, the stirrer furthercomprising a means for counterbalancing, such that when the motor ismoved to a position, the motor is maintained in that position by themeans for counterbalancing.
 6. The modular reactor system of claim 5,the stirrer further comprising a mount for mounting the motor, the mountcomprising the means for counterbalancing.
 7. The modular reactor systemof claim 6, wherein the means for counterbalancing comprises at leastone counterbalance arm.
 8. The modular reactor system of claim 7,wherein the at least one counterbalance arm is movable relative to themount.
 9. The modular reactor system of claim 6 wherein the means forcounterbalancing further comprises the motor, such that counterbalancingis provided by positioning the motor within the mount.
 10. The modularreactor system of claim 1, wherein the motor shaft is operably engagablewith a stir shaft to form a universal joint.
 11. The modular reactorsystem of claim 10, wherein the motor shaft comprises a telescopingportion.
 12. The modular reactor system of claim 11, wherein the stirshaft is sized so as to be insertable through a lid port on a reactorvessel.
 13. A modular reactor system comprising, a fixed backplane;motor movably coupled to the backplane; a motor shaft having a first endand a second end, wherein the first end is fixedly coupled to the motor;a reactor module having an interior wall that is configured to beremovably engaged with the backplane; a lid coupled to the interiorwall, wherein the interior wall and the lid define a reactor chamber,the lid has a port that is in fluid communication with the reactorchamber, and the port has an inner dimension; a stirrer shaft extendingthrough the port and having a first end positioned inside the reactorchamber and a second end positioned outside the chamber; and a stirringpropeller coupled to the first end of the stirrer shaft; wherein thesecond end of the stirrer shaft is configured to be removably coupled tothe second end of the motor shaft as the reactor module is engaged tothe backplane.
 14. The modular reactor system of claim 13, wherein themotor is coupled to a first end of a motor mount movable by rotationabout an axis, and the backplane is coupled to a second end of the motormount, such that the motor is movable about the axis with respect to thebackplane.
 15. The modular reactor system of claim 14, wherein the motormount comprises a counterbalance movable by rotation about the axis tobalance the motor with respect to the backplane.
 16. The modular reactorsystem of claim 14, wherein the motor mount is further movable byrotation about a second axis, such that the motor is movable about thesecond axis with respect to the backplane.
 17. The modular reactorsystem of claim 13, wherein the port has an inner diameter, and thestirrer shaft has an outer diameter that is approximately equal to theinner diameter of the port.
 18. The modular reactor system of claim 13,wherein the stirring propeller and the stirrer shaft are fabricated asan integral unit.
 19. The modular reactor system of claim 13, whereinthe motor shaft comprises a first section coupled to the motor, and asecond section slidably coupled to the first section and slidablyengagable with the second end of the stirrer shaft.
 20. The modularreactor system of claim 13, wherein the reactor module comprises anexterior wall coupled to and forming an anular region with the interiorwall.
 21. The modular reactor system of claim 20, wherein the exteriorwall has an inlet port in fluid communication with the anular region.22. The modular reactor system of claim 21, wherein the exterior wallhas an outlet port in fluid communication with the anular region and.23. The modular reactor system of claim 22, wherein the backplanecomprises an inlet port that is configured to be removably coupled tothe outlet port of the of the exterior wall of the reactor module as thereactor module is engaged to the backplane.
 24. The modular reactorsystem of claim 23, wherein the backplane comprises an outlet port thatis configured to be removably coupled to the inlet port of the of theexterior wall of the reactor module as the reactor module is engaged tothe backplane.
 25. The modular reactor system of claim 21, wherein thebackplane comprises an outlet port that is configured to be removablycoupled to the inlet port of the of the exterior wall of the reactormodule as the reactor module is engaged to the backplane.